4-Chloroaniline → 6-Chloro-N2-(4-chlorophenyl)pyrimidine-2,4-diamine

HRID 28546

反応式

HRID 28546 の反応式
Cl[C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[C:4]([Cl:9])[N:3]=1.[Cl:10][C:11]1[CH:17]=[CH:16][C:14]([NH2:15])=[CH:13][CH:12]=1>O1CCOCC1>[Cl:9][C:4]1[N:3]=[C:2]([NH:15][C:14]2[CH:16]=[CH:17][C:11]([Cl:10])=[CH:12][CH:13]=2)[N:7]=[C:6]([NH2:8])[CH:5]=1

参加物

4

反応物 2

HCID 78124-ChloroanilineHCID 823874-Pyrimidinamine, 2,6-dichloro-

生成物 1

HCID 860043166-Chloro-N2-(4-chlorophenyl)pyrimidine-2,4-diamine収率 42%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 2,6-dichloro-pyrimidin-4-yl-amine (0.492 g, 3.0 mmol) and 4-chloro-aniline (1.54 g, 12.0 mmol) in dioxane (25 ml) was heated under reflux for 3 hours. After cooled to room temperature, the mixture was filtered. Concentration of the filtrate under reduced pressure provided the crude product which was purified by flash chromatography on silica gel eluting with ethyl acetate-hexane (1:3) to provide 6-chloro-N*2*-(4-chloro-phenyl)-pyrimidine-2,4-diamine (0.32 g, 42% yield) as a white powder.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 3 hours
  3. filtrationthe mixture was filtered
  4. customConcentration of the filtrate under reduced pressure provided the crude product which
  5. customwas purified by flash chromatography on silica gel eluting with ethyl acetate-hexane (1:3)

出典と根拠

ORDレコード
ord-9eb5e6401f8f42b0be4eb920452e57df
出典データセット
uspto-grants-2008_09
特許番号
US07419984B2

関連ノート

読み込み中…